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Int. J. Mol. Sci. 2009, 10(11), 4977-4989; doi:10.3390/ijms10114977

Modification of Different Zirconium Propoxide Precursors by Diethanolamine. Is There a Shelf Stability Issue for Sol-Gel Applications?

1 Inorganic Materials Science, Faculty of Science & Technology, and Mesa+ Research Institute for Nanotechnology, University of Twente, P.O. Box 217, 7500 AE Enschede, The Netherlands 2 Department of Chemistry, SLU, Box 7015, 75007 Uppsala, Sweden
* Author to whom correspondence should be addressed.
Received: 12 October 2009 / Revised: 28 October 2009 / Accepted: 9 November 2009 / Published: 13 November 2009
(This article belongs to the Special Issue Sol-Gel Technique)
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Modification of different zirconium propoxide precursors with H2dea was investigated by characterization of the isolated modified species. Upon modification of zirconium n-propoxide and [Zr(OnPr)(OiPr)3(iPrOH)]2 with ½ a mol equivalent of H2dea the complexes [Zr2(OnPr)6(OCH2CH2)2NH]2 (1) and [Zr2(OnPr)2(OiPr)4(OCH2CH2)2NH]2 (2) were obtained. However, 1H-NMR studies of these tetranuclear compounds showed that these are not time-stable either in solution or solid form. The effect of this time instability on material properties is demonstrated by light scattering and TEM experiments. Modification of zirconium isopropoxide with either ½ or 1 equivalent mol of H2dea results in formation of the trinuclear complex, Zr{η3μ2-NH(C2H4O)2}3[Zr(OiPr)3]2(iPrOH)2 (3) countering a unique nona-coordinated central zirconium atom. This complex 3 is one of the first modified zirconium propoxide precursors shown to be stable in solution for long periods of time. The particle size and morphology of the products of sol-gel synthesis are strongly dependent on the time factor and eventual heat treatment of the precursor solution. Reproducible sol-gel synthesis requires the use of solution stable precursors.
Keywords: precursor chemistry; molecular structure; nona-coordinated zirconium precursor chemistry; molecular structure; nona-coordinated zirconium
This is an open access article distributed under the Creative Commons Attribution License (CC BY 3.0).

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Spijksma, G.I.; Blank, D.H.A.; Bouwmeester, H.J.M.; Kessler, V.G. Modification of Different Zirconium Propoxide Precursors by Diethanolamine. Is There a Shelf Stability Issue for Sol-Gel Applications? Int. J. Mol. Sci. 2009, 10, 4977-4989.

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